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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 14 (1991), S. 475-480 
    ISSN: 0935-6304
    Keywords: Coupled RPLC-GC ; Partially concurrent solvent evaporation ; Trapping column ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new technique for coupling reversed-phase liquid chromatography (RPLC) with gas chromatography is described. A fraction eluting from an RPLC column is trapped on a short column packed with polymeric adsorbent. After the mobile phase has been displaced with water, the analytes are desorbed with ethyl acetate. Following a delay time to enable the water to be flushed to waste, the ethyl acetate containing the analytes is introduced into the gas chromatograph under conditions suitable for partially concurrent solvent evaporation, i.e. below the solvent boiling point and at a rate just exceeding the evaporation rate. Post-column addition of water to the RPLC eluent helps to prevent breakthrough of compounds which are only modestly retained on the trapping column. The relationship between the capacity factors of the analytes on the trapping column and the required dilution factor is discussed. Polycyclic aromatic hydrocarbons are used as test compounds to study the system.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0935-6304
    Keywords: Coupled LC-GC-MS ; Aqueous sample ; s-Triazine Herbicides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Liquid chromatographic (LC) type trace enrichment is coupled online with capillary gas chromatography (GC) with mass spectrometric (MS) detection for the analysis of aqueous samples. A volume of 1-10 ml of an aqueous sample is preconcentrated on a trace-enrichment column packed with a polymeric stationary phase. After cleanup with HPLC-grade water the precolumn is dried with nitrogen and subsequently desorbed with ethyl acetate. A fraction of 60 μl is introduced on-line into a diphenyltetramethyldisilazane-deactivated retention gap under partially concurrent solvent evaporation conditions and using an early solvent vapor exit. The analytes are separated and detected by means of GC-MS. The potential of the LC-GC-MS system for monitoring organic pollutants in river and drinking water is studied. Target analysis is carried out with atrazine and simazine as model compounds; the detection limits achieved under full-scan and multiple ion detection conditions are 30 pg and 5 pg, respectively. Identification of unknown compounds (non-target analysis), is demonstrated using a river water sample spiked with 168 pollutants varying in polarity and volatility.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 13 (1990), S. 157-161 
    ISSN: 0935-6304
    Keywords: Coupled LC-GC ; Partially concurrent solvent evaporation ; Trace enrichment ; Surface water ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The feasibility of using ethyl acetate for the desorption of trace pollutants from a liquid chromatographic precolumn on-line into a diphenyltetramethyldisilazane-deactivated retention gap and, subsequently analysis by means of capillary gas chromatography has been demonstrated. First 5% of methanol are added to the water sample to prevent sorption of analytes onto parts of the preconcentration system. About 1 ml of this aqueous sample is injected onto a precolumn containing a polymeric stationary phase, using water-methanol (95:5, v/v) for transport and clean-up. The precolumn is desorbed with ethyl acetate and a fraction of 75 μl is injected on-line into the retention gap; separation is then achieved on a capillary CP Sil 19 column. No breakthrough of the test compounds was observed in the preconcentration step. The recovery was quantitative and the response obtained with flame ionization detection was linear in the range 0.1-100 ng/ml. The effect of varying the sorption flow rate on the recovery was studied. The system was applied to the analysis of river water.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 4
    ISSN: 0935-6304
    Keywords: LC-GC ; Aqueous samples ; Solid phase extraction ; Thermal desorption ; PTV ; Tenax GC© ; Reversed phase adsorbent ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new approach to the introduction of large aqueous samples into a gas chromatograph, solid phase extraction - thermal desorption, is presented. Carrier gas pushes the sample through a packed liner mounted in a programmed temperature vaporizer; analytes retained by the packing material are thermally desorbed after drying of the adsorbent. The sorption properties and thermal stability of some packing materials have been studied off-line. Tenax GC®, and octyl-modified silica silylated with diphenyltetramethyldisilazane to improve its thermal stability, appeared to be suitable materials.The drying period and the desorption temperature are critical for satisfactory performance of the method. When Tenax GC® is used as packing material, thermal desorption at 250°C for 15 min gives quantitative recovery for methyl esters up to hexacosanoic acid methyl ester. With the silylated octyl-modified silica, the application range is limited to the methyl esters of decanoic to octadecanoic acids.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 5
    ISSN: 1040-7685
    Keywords: solid phase extraction ; thermal desorption ; on-line ; aqueous samples ; gas chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A module for combined solid-phase extraction and thermal desorption (SPETD) was incorporated into a system for automated GC analysis. Solid-phase extraction of analytes from water could be carried out after injection of an aqueous sample of 100 μL either by a loop using the carrier gas for sample introduction or manually with a syringe. After drying of the stationary phase by the carrier gas at a high flow rate, thermal desorption could be carried out at temperatures up to 300-350°C. Suitable packing materials for the liner in the SPETD module, i.e., materials which efficiently trap the organic compounds from an aqueous solution and are sufficiently thermostable, include Tenax and carbon-based phases, as well as a silylated alkylmodified silica. With the latter, however, the problem of efficient drying after sorption still must be solved. Each phase has its own application range which, from among the analytes which are trapped during sorption, is determined at the volatile end by losses occurring during drying by helium purging, and at the nonvolatile end by losses due to incomplete release during thermal desorption. From this study (using n-alkanes, chlorobenzenes, and chlorophenols as test solutes), it appears that the Tenax phases, Tenax-TA and Tenax-GR, have the widest application range; essentially quantitative recoveries were obtained for C10 through C26 n-alkanes. The carbon-based phases appear to be useful for relatively volatile compounds, i.e., up to C19 n-alkanes. Each phase gave good recoveries for two test mixtures containing chlorobenzenes and chlorophenols dissolved in 100 μL of water at the 10 ppb level.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 6
    ISSN: 0935-6304
    Keywords: Coupled LC-GC ; Retention gap ; Variable splitter ; Partially concurrent solvent evaporation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A system is described which accelerates the solvent evaporation rate in the retention gap. The evaporation is due to a saturation effect of the carrier gas stream, and a considerable increase in evaporation rate is obtained by inserting a split outlet between the retention gap and the capillary separation column in the gas chromatograph. By varying the backpressure of the spliter device, the flow rate through the retention gap can be adjusted and so too the evaporation rate. The evaporation process was monitored by inserting a dectecter in the split outlet line. The technique was applied to the on-line LC trace enrichment/GC analysis of water containing a mixture of polycyclic aromatic hydrocarbons.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 7
    ISSN: 0935-6304
    Keywords: Solid-phase extraction-thermal desorption ; Gas chromatography ; Ion trap detection ; Tandem mass spectrometry ; Water samples ; Microcontaminants ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An improved set-up for solid-phase extraction with thermal desorption coupled on-line to gas chromatography (SPETD-GC) is presented. It includes a newly designed liner for a programmable temperature vaporizer (PTV) and an improved water elimination system. The SPETD procedure now includes a washing step with HPLC-grade water to prevent degradation of analytes due to interaction with remaining sample constituents. The system was used to analyze surface and tap water samples over a 4-month period. No decrease of chromatographic or trace-enrichment performance was observed, and a liner packed with Tenax GR could be used for at least 150 analyses. The SPETD module was coupled to GC with ion-trap detection for mass spectrometric (MS) and MS/MS detection. The linearity and repeatability of the procedure for several pesticides which were tested in the 0.5-10 μg/1 range were fully satisfactory (1 μg/1, RSD range 5-11%; n = 5). When using sample volumes of 0.1 ml only, detection limits were as low as 0. 1-0.2 μg/1. As an example, the confirmation and quantification of a suspected pesticide in a real-life sample using electron impact and positive chemical ionization in both the MS and MS/MS mode is shown.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 20 (1997), S. 363-368 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Solid-phase extraction ; Automation ; Water samples ; Acetylation ; Chlorophenols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An automated system for derivaatization was coupled on-line with solid-phase extraction-gas-chromatography (SPE-GC). The system was optimized for the determination of phenol and chlorinated phenols in aqueous samples. The test analytes were acetylated with acetic anhydride; proper buffering of the sample was a critical factor. Next, the phenol acetates were enriched on a SPE cartridge and transferred to a GC; two appraoaches were studied. In the first approach, the derivatives were enriched on disposable C18 cartridges (ASPEC type) and desorbed with methylacetate. Aan aliquot of the final eluate was injected on-line the GC by means of a loop-type interface. In the second approach, trace enrichment was performed on 10 × 2 mm i.d. LC-type precolumn packed with polystyrenedivinylbenzene copolymer (PLRP-S) this precolumn was dried with a mitrogen purge and the phenol acetates were desorbed with ethyl acetate which was injectedon-line into the retention gap of the GC under partially concurrent solvent evaporation (PCSE) conditions. The Derivatization-SPE-GC system which was based on the loop-type interface has the advantage of simplicity and easy operation, the main drawback is the impossibility to determine phenol acetates which elute prior to trichlorophenol acetates. With the derivatization-SPE-GC approach using PCSE-based desorption, even the most volatile analyte of the test series, phenol acetate, can be determined successfully. The entire procedure, including the derivatization step, was fully automated and integrated in one set-up. The precision data for the integrated on-line derivatization-SP-FID system were fully satisfactory, with RSD values of 1-12 % at the 1 μg/1 level. When a sample volume of 2.2 ml was analyzed, The detection limits for the chlorinated phenol acetates were in the 0.1-0.3 μg/1 range.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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